Process for matting textiles



Patented Nov. 24, 1942 PROCESS FOR MA'ITING TEXTILES Albert Landolt, Riehen,

Hans Benz. Basel, Swit and Gustav Widmer and lei-land, assignors to the firm Society of Chemical Industry in Basie,

Basel, Switzerland No Drawing.

6 Claims.

The water-insoluble urea-formaldehyde condensation products have been used repeatedly for improving textile fibers.

According to the process of Patent 1,734,516 these products are fixed on the fiber in the form of transparent, coherent condensation products. This imparts to the fiber inter alia the valuable property of being fast to creasing. According to such a process the individual fibers of the textile materials are covered with film-like coatings of the condensation products, so that the textile materials treated in such a manner, insofar as they consist of cellulose or regenerated cellulose, hardly show or do no longer show at all the cellulose reaction (a blue or black stain when spotted with an iodine solution in an aqueous solution of zinc chloride).

Water-insoluble urea-formaldehyde condensation products can also be used according to the processes of British Patents 469,688 and 467,480 in such a manner that pigment-like precipitates consisting of discrete particles are produced on the fiber, whereby valuable matt eifects are obtained. The proof that the insoluble ureaformaldehyde condensation products are formed on the fiber as subdivided, pigment-like precipitates, in contradistinction to the processes according to which coherent films are produced, is given by the fact that the textile materials treated in such a manner, provided they consist of cellu-' lose or regenerated cellulose, clearly show the above mentioned reaction with an iodine solution in an aqueous solution of zinc chloride.

For producing such matt effects one may start from various parent materials, for example from preformed water-insoluble condensation products. These are dissolved in acids, such as hydrochloric acid, phosphoric acid or formic acid. The

solutions thus formed are strongly diluted with water whereby matting baths are obtained in which the textile materials are treated. Alternatively, one may start from water-soluble addition products, such as monoand dimethylolurea, or from mixtures of the primary'parent materials, viz. urea and formaldehyde. Dilute solutions of such products to which acids are advantageously added as condensing agents, are then used as treating baths.

The treatment itself, regardless of whether one starts from preformed water-insoluble condensation products or whether the water-insoluble products are formed in the treating bath'only, is effected by two different methods.

One method consists in an exhausting process, 1. e. the textile materials are treated in dilute Application May 2. 1939, Serial No. In Switserland May '1, ma

baths wherein the insoluble condensation products are gradually separated, this separation being effected either by the precipitating action of water on the solutions of the preformed insoluble condensation products in acids, or by the condensing influence of acid on the water-soluble urea-formaldehyde addition products. This treatment in the bath itself is continued until the desired effect is attained.

According to the other method, working is effected by the padding principle, 1. e. the material is treated for a relatively short time with the concentrated matting liquor containing watersoluble urea-formaldehyde addition products or the mixture of urea and formaldehyde, then squeezed out, and passed through a second bath containing the acid, whereby the separation of the insoluble pigment takes place while matting the material. Padding can also be effected only once by adding a suitable acid to the matting liquor. After padding the material must then be left to lie until the matt effect is obtained.

The present process relates to a special form of carrying out the method of working designated in the foregoing as exhausting process, 1. e. only to that form of the exhausting process in which as parent materials water-soluble urea-formaldehyde addition products or mixtures of formaldehyde and urea are used. As mentioned above, in this method of working the matting baths are prepared with water-soluble addition products from urea and formaldehyde, such as monoand dimethylolurea or corresponding mixtures of urea and formaldehyde, and the condensation to the water-insoluble products is brought about by addition of small quantities of acids or condensing agents having an acid action, such as hydrochloric acid, sulfuric acid, phosphoric acid, bisulfate, zinc chloride and'the like. If this condensation takes place in the presence of textile materials the insoluble products which are graduv ally formed are precipitated on the textile materials with formation of the desired valuable fast matt effects, which are particularly fast to washing.

It has been found that in the form of operation described in the preceding paragraph for the production of pigment-like precipitates consisting of discreteparticles of insoluble urea-formaldehyde condensation products on textile materials, particularly favorable results are obtained when using, on the one hand, a matting bath containing monomethylolurea as water-soluble addition products, and, on the other hand, definite proportions of liquor,-that is to say such proportions wherein the quantity of the liquor does not exceed the -fold quantity of the material to be treated. Therefore, there are used baths which contain monomethylolurea or a mixture of urea with a water-soluble compound of urea which is correspondingly richer in formaldehyde, such as mixtures containing urea and dimethylolurea in molecular proportion 1:1. This latter procedure is particularly favorable on account of the easy producibility of the products. Moreover, it was not to be foreseen offhand that such a mixture would behave like the nonomethylolurea which is obtainable with more difficulty.

The method of working according to the present process proceeds in about the following manner:

A matting bath is prepared by dissolving monomethylolurea or an approximately equimolecular mixture of dimethylolurea and urea in water and bringing the solution to the indicated concentration, while simultaneously acidifying the same. The material to be matted is then handled in the bath until the desired matting effect is attained which is brought about by the precipitation on the fiber of the urea-formaldehyde condensation products formed in the acid solution. Thus it is possible, for example in a matting liquor containing per liter 7.5 grams of an approximately equimolecular mixture of dimethylolurea and urea and 3.5 grams of hydrogen chloride, to impart a strong matting to viscose rayon in the course of about hour in a bath which remain. entirely clear, the ratio of material to liquor being 1:10. A sample of the matting liquor withdrawn before the viscose is introduced shows however that after the acid has acted on the liquor for not more than 10 minutes, there is formed a white precipitate which is even increased on longer standing.

The mattings obtained are not only stable to the treatment with water, but also to hot soap solutions, such as are used in the textile improving industry.

The new process permits the matting of lustrous fibers before dyeing, which may be of advantage in many cases. The yield of matting increases with greater liquor concentrations. Working with too long a liquor, for example with a liquor which essentially exceeds the proportion 1:15, is therefore uneconomical. In many cases the handle of the material can be improved by using a softening agent.

The following examples illustrate the invenv tion Example 1 a fairly strong matting. When the ratio of goods 6 to liquor is 1:8 there is obtained a stronger matting.

Example 2 Viscose rayon yarn is matted for hour at 25 C. in a liquor which, calculated on the weight of the yarn, contains 7.5 per cent of an approximately equimolecular mixture of dimethylolurea and urea, and 12 per cent of hydrochloric acid of 20 B., the goods to liquor ratio being 1:10. The

matting liquor remains clear as water during the treatment; the viscose is strongly matted after rinsing and drying. An even stronger matting can be obtained by reducing the liquor ratio.

When treating otherfibers in this manner, for example naturalsilk or mercerized cotton Or textile materials consistingof mixtures of various fabrics, such as artificial silk from regenerated or acetylated cellulose, matt effects are also obtained.

Example 3 Viscose rayon yarn which has been matter for hour at ordinary temperature with 15 per cent of an approximately equimolecular mixture of dimethylolurea and urea and 12 per cent of hydrochloric acid of 20 B., the goods to liquor ratio being 1:10, shows a very strong matting, similar to the matting produced on rayon which has been matted in the viscose mass with titanium dioxide or similar pigments.

When matting in a manner similar to that indicated in the preceding paragraph, but using 12 per cent of formic acid of per cent strength calculated on the weight of the yarn instead of the hydrochloric acid, a matting of medium strength is obtained.

Example 4 Acetate rayon is treated on a mechanical reel for hour at 25 C. in a liquor described in Example 2. The acetate rayon is matted in this manner, and the matting becomes fast to soaping also here. The matting of acetate rayon in cold baths has the advantage over the known hot matting in the presence of phenol or pine oil that the fibrous material is largely protected.

Example 5 Viscose rayon yarn is treated for hour a. 30 C. with 7 .5 per cent of the equimolecular mixture from dimethylolurea and urea and 16 per cent of hydrochloric acid of 20 B., the goods to liquor ratio being 1: 15. There is obtained a matting of medium strength.

Example 6 Rayon yarn is matted at 50 C. as prescribed in Example 2, the material being treated on a mechanical reel. There is obtained a strong matting.

Example 7 Viscose rayon piece goods are dyed with the following dyestuif combination:

0.048 per cent of Chlorantine Fast Orange T4RLL (Schultz Jul., 7th edition, 1st supp]. vol., page 79) and 0.006 per cent of Chlorantine Fast Red SBLL (Schultz Jul., 7th edition, vol 2, page 48) and 10 per cent of Glaubers salt (calculated on the fibrous material). The material is then rinsed and matted on a mechanical reel as described in Example 2. The rayon is completely matt. Strong mattings are also obtained on socalled Interlock and Tweed materials made from strongly twisted rayon threads.

Example 8 Copper rayon tricot is matted on a reel as described in Example 2 and then dyed with 6 per cent of Direct Chromium Black Blue B (Schultz Jul., 7th edition, 1st suppl. vol., page 89) in a bath containing Glaubers salt. There is obtained a dark blue matted dyeing.

What we claim is:

1. A process for matting textile material in a bath of matting liquor, which comprises immersing the material to be treated in the said bath, and forming a water-insoluble urea-formaldehyde condensation product as a pigment-like precipitate in discrete particles in the bath and on the textile material therein by the action of precipitating acid in the bath on a water-soluble urea-formaldehyde condensation product, the

matting liquor containing the water-soluble urea-formaldehyde condensation product in the form of a member of the group consisting of monomethylolurea and an approximately equimolecular mixture of dimethylolurea and urea, and the ratio of textile material to liquor not exceeding 1:15,

2. A process for matting textile material in a bath of matting liquor, which comprises immersing the material to be treated in the said bath, and forming a water-insoluble urea-formaldehyde condensation product as a pigmentlike precipitate in discrete particles in the bath and on the textile material therein by the action of precipitating acid in the bath on a watersoluble urea-formaldehyde condensation product, the matting liquor containing the watersoluble urea-formaldehyde condensation product in the form of methylolurea, and the ratio of textile material to liquor not exceeding 1:15;

3. A process for matting textile material in a bath of matting liquor, which comprises immersing the material to be treated in the said bath, and foming a water-insoluble urea-formaldehyde condensation product as a pigment-like precipitate in discrete particles in the bath and on the textile material therein by the action of precipitating acid in the bath on a water-soluble urea-formaldehyde condensation product, the matting liquor containing the water-soluble urea-formaldehyde condensation product in the form of methylolurea, and the ratio of textilev material to liquor not exceeding 1:10. I

4. A process for matting textile material in. a bath of matting liquor, which comprisesimmersing the material to be treated in the said bath, and forming a water-insoluble urea-forma1de-' hyde condensation product as a pigment-like precipitate in discrete on the textile material therein by the action of hydrochloric acid in the bath on a water-soluble urea-formaldehyde condensation product, the matting liquor containing the water-soluble urea-formaldehyde condensation product in the form of a member of the group consisting of monomethylolurea and an approximately equimolecular mixture of dimethylolurea and urea, and the ratio of textile material to liquor not exceeding 1:15.

5. A process for matting textile material in a bath of matting liquor, which comprises immersing the material to be treated in the said bath,

and forming a. water-insoluble urea-formaldehyde condensation product as a pigment-like precipitate in discrete particles in the bath and on the textile material therein by the action of phosphoric acid in the bath on a water-soluble urea-formaldehyde condensation product, the matting liquor containing the water-soluble urea-formaldehyde condensation product in the form of a member of the group consisting of monomethylolurea and an approximately equimolecular mixture of dimethylolurea and urea, and the ratio of textile material to liquor not exceeding 1:15.

6. A process for matting textile material in a bath of matting liquor, which comprises immersing the material to be treated in the said bath, and forming a water-insoluble urea-formaldehyde condensation product as a pigment-like precipitate in discrete particles in the bath and on the textile material therein by the action of sulfuric acid in the bath on a water-soluble ureaformaldehyde condensation product, the matting liquor containing the water-soluble urea-formaldehyde condensation product in the form of a member of the group consisting of monomethylolurea and an approximately equimolecular mixture of dimethylolurea and urea, and the ratio of textile material to liquor not exceeding 1: 5-

ALBERT LANDOLT. GUSTAV WIDMER. HANS BENZ.

particles in the bath and 

